TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석
Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA dervative
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Abstract
Early diagnosis and medical intervention are critical for the treatment of patients withmetabolic disorders. A rapid analytical method was developed for simultaneous quantification ofhigh sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paperurine specimens were dried under nitrogen after being fortified with internal standard (tropate)in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicatorreagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative. Corresponding authorPhone : +82+(0)2-901-8387 Fax : +82+(0)2-997-1990E-mail: hyeran1@duksung.ac.kr108 . . .Analytical Science & Technologyfor amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bis-trifluoroacetamide were consecutively added and heated for 15-20 min at 65oC-70oC, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic rangeshowed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limitof 80-900 ng in urine. Corelation coefficient of regression line was 0.994-0.998. When the methodwas applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolicdisorder. The study showed that the developed method could be the method of choices in rapidand sensitive screening for organic aciduria and amino acidopathy.
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